JP7087282B2 - Surface inspection method of electrolytic copper foil and manufacturing method of electrolytic copper foil - Google Patents
Surface inspection method of electrolytic copper foil and manufacturing method of electrolytic copper foil Download PDFInfo
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- 238000000034 method Methods 0.000 title claims description 61
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
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- Electroplating Methods And Accessories (AREA)
Description
本発明は、電解銅箔の表面検査方法及び電解銅箔の製造方法に関する。 The present invention relates to a method for surface inspection of electrolytic copper foil and a method for producing electrolytic copper foil.
プリント配線板用電解銅箔は、一般的に、一方の表面が平滑な光沢面であり、他方の表面がプリプレグ等との密着性を確保するために、粗化処理が施された粗化処理面となっている。
この粗化処理は、通常、粗化処理前の電解銅箔のマット面（凹凸が大きい面）に銅等の粒子（以下、「粗化粒子」ともいう）を電析させる処理である。粗化処理前の電解銅箔の表面において、高い凸部が存在していたり、傷等によって表面形状が通常と異なっていた場合、電析時の電流密度が局所的に高くなることから、粗化粒子が局所的に多く析出してしまうことがある。このような現象は、粗化異常又は異常突起と呼ばれ、通常、その大きさは、直径が５～１００μｍ、高さが２～３０μｍの範囲で発生することが多い。粗化異常又は異常突起が発生した箇所（以下、「粗化異常部」ともいう）が存在する銅張積層板を回路加工した場合、粗化異常部がエッチングで溶解されず、回路欠陥となったり、絶縁信頼性が損なわれるといった問題が生じる。
In general, one surface of electrolytic copper foil for printed wiring boards is a smooth glossy surface, and the other surface is roughened in order to ensure adhesion to a prepreg or the like. It is a face.
This roughening treatment is usually a treatment of electrodepositing particles such as copper (hereinafter, also referred to as "roughened particles") on the matte surface (surface having large irregularities) of the electrolytic copper foil before the roughening treatment. If there are high protrusions on the surface of the electrolytic copper foil before the roughening treatment, or if the surface shape is different from the normal one due to scratches, etc., the current density at the time of electrodeposition increases locally, so that the roughening is performed. A large amount of chemical particles may be deposited locally. Such a phenomenon is called a roughening abnormality or anomalous protrusion, and its size usually occurs in the range of 5 to 100 μm in diameter and 2 to 30 μm in height. When a copper-clad laminate having a portion where an abnormal roughening or an abnormal protrusion occurs (hereinafter, also referred to as an "abnormal roughening portion") is circuit-processed, the abnormal roughening portion is not melted by etching and becomes a circuit defect. In addition, there are problems such as impaired insulation reliability.
電解銅箔の粗化処理面の品質検査方法としては、表面粗さ測定、電子顕微鏡、実体顕微鏡、ＣＣＤカメラ等による観察などが行われている（例えば、特許文献１参照）。 As a method for inspecting the quality of the roughened surface of the electrolytic copper foil, surface roughness measurement, observation with an electron microscope, a stereomicroscope, a CCD camera, or the like is performed (see, for example, Patent Document 1).
しかしながら、表面粗さ測定、電子顕微鏡等による検査方法は、極めて小さい面積しか測定できないため、粗化異常部を検出することが困難である。
また、実体顕微鏡、ＣＣＤカメラ等による観察は、粗化処理面の色調がほぼ均一であること、粗化異常部のサイズが小さいこと等に起因して、粗化異常部の検出及び判別が困難であるという課題がある。
However, it is difficult to detect an abnormal roughness portion because the surface roughness measurement, the inspection method using an electron microscope, or the like can measure only an extremely small area.
Further, when observing with a stereomicroscope, a CCD camera, etc., it is difficult to detect and discriminate the roughened abnormal portion due to the fact that the color tone of the roughened abnormal portion is almost uniform and the size of the roughened abnormal portion is small. There is a problem that it is.
本発明は、電解銅箔の粗化処理面に存在する粗化異常部を、容易かつ高精度で検出することができる電解銅箔の表面検査方法、及び該検査方法を適用した電解銅箔の製造方法を提供することを目的とする。 The present invention is a surface inspection method for an electrolytic copper foil capable of easily and with high accuracy to detect an abnormal roughening portion existing on a roughened surface of the electrolytic copper foil, and an electrolytic copper foil to which the inspection method is applied. The purpose is to provide a manufacturing method.
本発明者らは、上記課題を解決すべく鋭意検討を重ねた結果、電解銅箔の粗化処理面に塗膜を形成し、該塗膜を観察することで、容易かつ高精度で粗化異常部を検出できることを見出し、本発明を完成するに至った。すなわち、本発明は、以下の［１］～［８］に関する。
［１］粗化処理面を有する電解銅箔の表面検査方法であって、前記電解銅箔の粗化処理面上に、粗化異常部観察用物質の塗膜を形成する工程と、前記塗膜を観察して粗化異常部を検出する工程と、を有する電解銅箔の表面検査方法。
［２］前記粗化異常部観察用物質が、２５℃で液状の物質である、上記［１］に記載の電解銅箔の表面検査方法。
［３］前記２５℃で液状の物質が、親油性の液体である、上記［２］に記載の電解銅箔の表面検査方法。
［４］前記塗膜を形成する工程が、前記電解銅箔の粗化処理面に前記粗化異常部観察用物質を噴霧して塗膜を形成する工程である、上記［１］～［３］のいずれかに記載の電解銅箔の表面検査方法。
［５］前記電解銅箔が、プリント配線板用電解銅箔である、上記［１］～［４］のいずれかに記載の電解銅箔の表面検査方法。
［６］前記塗膜の観察を、光学顕微鏡を用いて行う、上記［１］～［５］のいずれかに記載の電解銅箔の表面検査方法。
［７］電解銅箔の少なくとも一方の面を粗化処理する工程と、得られた粗化処理後の電解銅箔に対して、上記［１］～［６］のいずれかに記載の電解銅箔の表面検査方法を実施して良否を判定する工程を含む、電解銅箔の製造方法。
［８］前記粗化処理が、前記電解銅箔の表面に銅を析出させる処理である、上記［７］に記載の電解銅箔の製造方法。
As a result of diligent studies to solve the above problems, the present inventors have formed a coating film on the roughened surface of the electrolytic copper foil, and by observing the coating film, roughening is easy and highly accurate. We have found that an abnormal part can be detected, and have completed the present invention. That is, the present invention relates to the following [1] to [8].
[1] A method for surface inspection of an electrolytic copper foil having a roughened surface, wherein a coating film of a material for observing an abnormal roughening portion is formed on the roughened surface of the electrolytic copper foil, and the coating. A method for surface inspection of an electrolytic copper foil, which comprises a step of observing a film and detecting an abnormal roughening portion.
[2] The method for surface inspection of an electrolytic copper foil according to the above [1], wherein the substance for observing an abnormal roughening portion is a substance that is liquid at 25 ° C.
[3] The method for surface inspection of an electrolytic copper foil according to the above [2], wherein the liquid substance at 25 ° C. is a lipophilic liquid.
[4] The step of forming the coating film is a step of spraying the substance for observing the abnormal roughening portion on the roughened surface of the electrolytic copper foil to form the coating film, as described above [1] to [3]. ] The surface inspection method for the electrolytic copper foil according to any one of.
[5] The method for surface inspection of an electrolytic copper foil according to any one of the above [1] to [4], wherein the electrolytic copper foil is an electrolytic copper foil for a printed wiring board.
[6] The method for surface inspection of an electrolytic copper foil according to any one of the above [1] to [5], wherein the coating film is observed using an optical microscope.
[7] The electrolytic copper according to any one of [1] to [6] above, with respect to the step of roughening at least one surface of the electrolytic copper foil and the obtained electrolytic copper foil after the roughening treatment. A method for producing an electrolytic copper foil, which comprises a step of performing a surface inspection method of the foil and determining the quality.
[8] The method for producing an electrolytic copper foil according to the above [7], wherein the roughening treatment is a treatment for precipitating copper on the surface of the electrolytic copper foil.
本発明によれば、電解銅箔の粗化処理面に存在する粗化異常部を、容易かつ高精度で検出することができる電解銅箔の表面検査方法、及び該検査方法を適用した電解銅箔の製造方法を提供することができる。 According to the present invention, a surface inspection method for an electrolytic copper foil capable of easily and with high accuracy to detect an abnormal roughening portion existing on the roughened surface of the electrolytic copper foil, and an electrolytic copper to which the inspection method is applied. A method for producing a foil can be provided.
以下、本発明の一実施形態について詳述するが、本発明は以下の実施形態に限定されるものではない。
なお、以下の実施形態において、粗化処理前の電解銅箔を「未処理電解銅箔」と称することがあり、単に「電解銅箔」という場合は、「粗化処理後の電解銅箔」を指すものとする。
Hereinafter, one embodiment of the present invention will be described in detail, but the present invention is not limited to the following embodiments.
In the following embodiments, the electrolytic copper foil before the roughening treatment may be referred to as "untreated electrolytic copper foil", and the term "electrolytic copper foil" is simply referred to as "electrolytic copper foil after roughening treatment". Shall point to.
［電解銅箔の表面検査方法］
本実施形態の電解銅箔の表面検査方法は、粗化処理面を有する電解銅箔の表面検査方法であって、前記電解銅箔の粗化処理面上に、粗化異常部観察用物質の塗膜を形成する工程（以下、「塗膜形成工程」ともいう）と、前記塗膜を観察して粗化異常部を検出する工程（以下、「観察工程」ともいう）と、を有する電解銅箔の表面検査方法である。
本実施形態の検査方法において、粗化異常部観察用物質は、粗化処理面に形成された粗化粒子間の微細な隙間に侵入し、表面張力によって粗化処理面上に塗膜が形成される。該塗膜が形成された部分は色調が殆ど一定となるが、粗化異常部では、正常な部分と比較して粗化粒子の高さが高いことに起因して塗膜が形成されなかったり、塗膜が薄くなり、色調、形状等が正常な部分とは異なって見える。このため、塗膜を形成した粗化処理面を、実体顕微鏡等で観察することで、塗膜を形成していない場合よりも、粗化異常部の検出、判別等を容易かつ高精度に行うことができる。
[Surface inspection method for electrolytic copper foil]
The method for inspecting the surface of the electrolytic copper foil of the present embodiment is a method for inspecting the surface of the electrolytic copper foil having a roughened surface, and the material for observing the abnormal roughening portion is on the roughened surface of the electrolytic copper foil. Electrolysis having a step of forming a coating film (hereinafter, also referred to as “coating film forming step”) and a step of observing the coating film to detect an abnormal roughening portion (hereinafter, also referred to as “observation step”). This is a surface inspection method for copper foil.
In the inspection method of the present embodiment, the substance for observing the abnormal roughening portion penetrates into the fine gaps between the roughened particles formed on the roughened surface, and a coating film is formed on the roughened surface due to surface tension. Will be done. The color tone of the portion where the coating film is formed is almost constant, but in the roughened abnormal portion, the coating film may not be formed due to the higher height of the roughened particles as compared with the normal portion. , The coating film becomes thin, and the color tone, shape, etc. look different from the normal part. Therefore, by observing the roughened surface on which the coating film is formed with a stereomicroscope or the like, it is easier and more accurate to detect and discriminate the roughening abnormality portion than in the case where the coating film is not formed. be able to.
＜電解銅箔＞
本実施形態の検査方法を適用する電解銅箔は、粗化処理面を有する電解銅箔である。
本実施形態の検査方法によると、回路欠陥等の原因となる粗化異常部を容易かつ高精度で検出できるため、本実施形態の検査方法は、特に、プリント配線板用銅張積層板等に用いられる、プリント配線板用電解銅箔に対して好適である。
電解銅箔が有する粗化処理面の表面粗さＲｚは、特に限定されず、例えば、０．５～２０μｍであってもよく、また、回路のファインピッチ化の観点からは、０．５～６μｍであってもよい。電解銅箔の表面粗さＲｚは、ＪＩＳ Ｂ０６０１：１９８２に準拠して測定することができる。
電解銅箔の厚さは、例えば、１～１００μｍであってもよく、電解銅箔の機械強度及びプリント配線板の薄型化の観点からは、５～５０μｍであってもよい。
次に、本実施形態の検査方法を、各工程順に説明する。
<Electrolytic copper foil>
The electrolytic copper foil to which the inspection method of the present embodiment is applied is an electrolytic copper foil having a roughened surface.
According to the inspection method of the present embodiment, a roughened abnormal portion that causes a circuit defect or the like can be detected easily and with high accuracy. Therefore, the inspection method of the present embodiment is particularly applied to a copper-clad laminate for a printed wiring board or the like. It is suitable for the electrolytic copper foil for printed wiring boards used.
The surface roughness Rz of the roughened surface of the electrolytic copper foil is not particularly limited, and may be, for example, 0.5 to 20 μm, and from the viewpoint of fine pitching of the circuit, 0.5 to 20 μm. It may be 6 μm. The surface roughness Rz of the electrolytic copper foil can be measured according to JIS B0601: 1982.
The thickness of the electrolytic copper foil may be, for example, 1 to 100 μm, and may be 5 to 50 μm from the viewpoint of the mechanical strength of the electrolytic copper foil and the thinning of the printed wiring board.
Next, the inspection method of this embodiment will be described in the order of each process.
＜塗膜形成工程＞
塗膜形成工程は、電解銅箔の粗化処理面上に、粗化異常部観察用物質の塗膜を形成する工程である。なお、塗膜形成工程の前に、必要に応じて、電解銅箔を観察し易い大きさに適宜加工しておいてもよい。
<Coating film forming process>
The coating film forming step is a step of forming a coating film of a substance for observing an abnormal roughening portion on the roughened surface of the electrolytic copper foil. If necessary, the electrolytic copper foil may be appropriately processed to a size that makes it easy to observe before the coating film forming step.
（粗化異常部観察用物質）
粗化異常部観察用物質は、前述の通り、粗化処理面上に塗膜を形成し、粗化異常部の観察を容易にするために使用されるものであり、その目的を達成できるものであれば特に限定されない。
粗化異常部観察用物質は、通常、電解銅箔と反応性を有さず、かつ電解銅箔を溶解しないものであり、取り扱い性の観点から、２５℃で液状である物質が好ましい。また、２５℃で液状である物質は、表面張力が小さく、電解銅箔の粗化処理面上に塗膜を形成し易い観点から、親油性の液体であることが好ましい。
粗化異常部観察用物質の具体例としては、やし油等の植物油；パラフィン系、ナフテン系等の鉱物油；エステル化合物、ポリαオレフィン、ポリオールエステル化合物、アルキル置換ジフェニルエーテル、ポリフェニルエーテル、フッ素オイル、シリコーンオイル等の合成油；水；その他の有機溶剤；無機物質などが挙げられる。これらは１種を単独で用いてもよく、２種以上を混合して用いてもよい。これらの中でも、親油性の液体であり、電解銅箔上に塗膜を形成し易い観点から、油類（オイル）が好ましく、鉱物油及び合成油からなる群から選ばれる１種以上がより好ましく、鉱物油がさらに好ましい。さらに、上記の物質に対して、防錆添加剤等の特定の機能を付与した添加剤を適宜含ませたものであってもよい。
粗化異常部観察用物質として使用できる油類としては、例えば、市販品の潤滑油として入手することもできる。
(Substance for observing abnormal roughening)
As described above, the substance for observing the abnormally roughened portion is used to form a coating film on the roughened surface to facilitate the observation of the abnormally roughened portion, and can achieve the purpose. If so, it is not particularly limited.
The substance for observing the abnormal roughening portion usually does not have reactivity with the electrolytic copper foil and does not dissolve the electrolytic copper foil, and from the viewpoint of handleability, a substance that is liquid at 25 ° C. is preferable. Further, the substance that is liquid at 25 ° C. is preferably a lipophilic liquid from the viewpoint that the surface tension is small and a coating film is easily formed on the roughened surface of the electrolytic copper foil.
Specific examples of substances for observing abnormally roughened parts include vegetable oils such as coconut oil; paraffin-based and naphthen-based mineral oils; ester compounds, poly α-olefins, polyol ester compounds, alkyl-substituted diphenyl ethers, polyphenyl ethers, and fluorine. Synthetic oils such as oils and silicone oils; water; other organic solvents; inorganic substances and the like. One of these may be used alone, or two or more thereof may be mixed and used. Among these, oils are preferable from the viewpoint of being an oil-based liquid and easily forming a coating film on the electrolytic copper foil, and one or more selected from the group consisting of mineral oil and synthetic oil is more preferable. , Mineral oil is more preferred. Further, the above-mentioned substance may appropriately contain an additive having a specific function such as a rust preventive additive.
As the oils that can be used as a substance for observing an abnormally roughened portion, for example, they can be obtained as commercially available lubricating oils.
粗化異常部観察用物質の２５℃における動粘度は、粗化処理面の微小な空隙等にも侵入し易くする観点、及び粗化処理面上に塗膜を保持され易くする観点から、２～７０ｍｍ２／ｓが好ましく、５～５０ｍｍ２／ｓがより好ましい。
粗化異常部観察用物質の沸点は、短時間に揮発することを抑制し、作業性を良好にする観点から、常圧下において、１５０℃以上が好ましく、２００℃以上がより好ましく、２５０℃以上がさらに好ましい。粗化異常部観察用物質の沸点の上限は特に制限はないが、例えば、５００℃以下であってもよく、４００℃以下であってもよい。
粗化異常部観察用物質は色調は、特に限定されないが、汎用性の観点から、透明であることが好ましい。
The kinematic viscosity of the material for observing the abnormal roughening portion at 25 ° C. is 2 from the viewpoint of facilitating the penetration into minute voids and the like on the roughened surface and from the viewpoint of facilitating the retention of the coating film on the roughened surface. It is preferably ~ 70 mm 2 / s, more preferably 5 to 50 mm 2 / s.
The boiling point of the material for observing the abnormally roughened portion is preferably 150 ° C. or higher, more preferably 200 ° C. or higher, and more preferably 250 ° C. or higher under normal pressure from the viewpoint of suppressing volatilization in a short time and improving workability. Is even more preferable. The upper limit of the boiling point of the material for observing the abnormal roughening portion is not particularly limited, but may be, for example, 500 ° C. or lower, or 400 ° C. or lower.
The color tone of the substance for observing the abnormally roughened portion is not particularly limited, but it is preferably transparent from the viewpoint of versatility.
（塗膜の形成）
電解銅箔の粗化処理面上に粗化異常部観察用物質の塗膜を形成する方法としては、例えば、粗化異常部観察用物質を、電解銅箔の粗化処理面上に塗工する方法、粗化異常部観察用物質を電解銅箔の粗化処理面上に噴霧する方法、電解銅箔を粗化異常部観察用物質に浸漬した後、取り出す方法などが挙げられる。これらの中でも、作業性の観点から、粗化異常部観察用物質を電解銅箔の粗化処理面上に噴霧する方法が好ましい。なお、粗化異常部観察用物質が常温で固体である場合には、粗化異常部観察用物質を加熱する方法、液状の物質と混合して溶液とする方法等によって液状にして、前記方法に適用することが好ましい。
(Formation of coating film)
As a method of forming a coating film of the material for observing the abnormal roughening portion on the roughened surface of the electrolytic copper foil, for example, the substance for observing the abnormal roughening portion is applied on the roughened surface of the electrolytic copper foil. A method of spraying a substance for observing an abnormally roughened portion on a roughened surface of an electrolytic copper foil, a method of immersing an electrolytic copper foil in a substance for observing an abnormally roughened portion, and then taking it out. Among these, from the viewpoint of workability, a method of spraying a substance for observing an abnormally roughened portion on the roughened surface of the electrolytic copper foil is preferable. When the substance for observing the abnormally roughened portion is solid at room temperature, the substance for observing the abnormally roughened portion is liquefied by a method of heating the substance for observing the abnormally roughened portion, a method of mixing with a liquid substance to form a solution, or the like, and the above method. It is preferable to apply to.
＜観察工程＞
観察工程は、塗膜形成工程で形成した塗膜を観察して粗化異常部を検出する工程である。
粗化異常部観察用物質の塗膜は、粗化異常部において、塗膜が形成されなかったり、塗膜が薄くなり、色調、形状等の外観が正常な部分とは異なって見えるため、観察によって、容易に粗化異常部を検出することができる。
塗膜の観察方法は特に限定されないが、作業性の観点から、光学顕微鏡を用いることが好ましく、実体顕微鏡を用いることがより好ましい。
粗化異常部は、前記顕微鏡等を介して目視することで検出することができるが、画像解析装置等を用いて自動カウントさせてもよい。
<Observation process>
The observation step is a step of observing the coating film formed in the coating film forming step to detect an abnormal roughening portion.
The coating film of the material for observing the abnormal roughening part is observed because the coating film is not formed or the coating film becomes thin in the abnormal roughening part, and the appearance such as color tone and shape looks different from the normal part. Therefore, the roughened abnormal portion can be easily detected.
The method of observing the coating film is not particularly limited, but from the viewpoint of workability, it is preferable to use an optical microscope, and it is more preferable to use a stereomicroscope.
The roughening abnormality portion can be detected by visual inspection through the microscope or the like, but it may be automatically counted by using an image analysis device or the like.
塗膜観察時の圧力は、粗化異常部を検出し易い条件を適宜選択すればよいが、作業性の観点からは、常圧下で実施することが好ましい。
塗膜観察時の温度は、粗化異常部を検出し易い条件を適宜選択すればよいが、作業性の観点からは、０～１００℃が好ましく、１５～５０℃がより好ましく、室温がさらに好ましく、常温（２５℃）が特に好ましい。
なお、本明細書において、室温とは、加熱、冷却等の温度制御なしの雰囲気温度をいうものとし、一般に、１５～２５℃程度であるが、天候、季節等によって変わり得るため、該範囲に限定されるものではない。
The pressure at the time of observing the coating film may be appropriately selected under conditions that make it easy to detect the abnormally roughened portion, but from the viewpoint of workability, it is preferable to carry out the pressure under normal pressure.
The temperature at the time of observing the coating film may be appropriately selected under conditions that make it easy to detect the abnormally roughened portion, but from the viewpoint of workability, 0 to 100 ° C. is preferable, 15 to 50 ° C. is more preferable, and room temperature is further preferable. Room temperature (25 ° C.) is preferable, and room temperature (25 ° C.) is particularly preferable.
In the present specification, the room temperature means an atmospheric temperature without temperature control such as heating and cooling, and is generally about 15 to 25 ° C. However, since it may change depending on the weather, season, etc., it is within the range. Not limited.
［電解銅箔の製造方法］
本実施形態の電解銅箔の製造方法は電解銅箔の少なくとも一方の面を粗化処理する工程（以下、「粗化処理工程」ともいう）と、得られた粗化処理後の電解銅箔に対して、前記本実施形態の電解銅箔の表面検査方法を実施して良否を判定する工程（以下、「検査工程」ともいう）を含む、電解銅箔の製造方法である。
[Manufacturing method of electrolytic copper foil]
The method for producing an electrolytic copper foil of the present embodiment includes a step of roughening at least one surface of the electrolytic copper foil (hereinafter, also referred to as “roughening treatment step”) and the obtained electrolytic copper foil after the roughening treatment. On the other hand, it is a method for producing an electrolytic copper foil, which comprises a step of carrying out the surface inspection method of the electrolytic copper foil of the present embodiment and determining the quality (hereinafter, also referred to as “inspection step”).
＜粗化処理工程＞
粗化処理工程は、電解銅箔の少なくとも一方の面を粗化処理する工程である。
本実施形態の製造方法において、粗化処理に供する未処理電解銅箔は、公知の方法によって製造することができる。その一例としては、硫酸銅水溶液等の電解液中に、ＳＵＳ、チタン等の陰極回転ドラムと、該陰極回転ドラムに対して同心円状に鉛等の陽極を配置し、電解液を供給させつつ両極間に電流を流して電解液を電解させ、該陰極回転ドラムの表面に所定の厚さに銅を析出させ、この析出した銅を連続的に剥がして巻取る方法が挙げられる。この方法によると、通常は、陰極回転ドラム側の表面が光沢面となり、電解液と接していた面がマット面（凹凸面）となる。マット面の表面粗さＲｚは、製造容易性及びファインピッチ化の観点から、０．０１～２μｍであることが好ましい。
<Roughening process>
The roughening treatment step is a step of roughening at least one surface of the electrolytic copper foil.
In the production method of the present embodiment, the untreated electrolytic copper foil to be subjected to the roughening treatment can be produced by a known method. As an example, a cathode rotating drum such as SUS or titanium and an anode such as lead are arranged concentrically with respect to the cathode rotating drum in an electrolytic solution such as an aqueous solution of copper sulfate, and both poles are supplied while supplying the electrolytic solution. Examples thereof include a method in which a current is passed between them to electrolyze the electrolytic solution, copper is deposited on the surface of the cathode rotating drum to a predetermined thickness, and the precipitated copper is continuously peeled off and wound. According to this method, the surface on the cathode rotating drum side is usually a glossy surface, and the surface in contact with the electrolytic solution is a matte surface (uneven surface). The surface roughness Rz of the matte surface is preferably 0.01 to 2 μm from the viewpoint of ease of manufacture and fine pitching.
次に、未処理電解銅箔に対して、粗化処理を行う。
粗化処理は、例えば、硫酸銅等の電解液を電解させて、未処理電解銅箔のマット面（凹凸面）側に、銅を含む粗化粒子を均一に析出させる、めっき法によって行うことができる。より具体的には、未処理電解銅箔を陰極とし、対極に不溶性陽極を配置して、例えば、液温２０～４０℃の硫酸銅等の銅めっき液を用い、平均陽極電流密度５Ａ／ｄｍ２～４０Ａ／ｄｍ２の条件で電解させ、未処理電解銅箔のマット面に粗化粒子を析出させることができる。さらに、上記の操作を必要に応じて複数回実施してもよい。
前記粗化処理工程によって形成する粗化粒子は、通常は、銅を含むものであり、銅以外の元素として、モリブデン（Ｍｏ）、ニッケル（Ｎｉ）、コバルト（Ｃｏ）、鉄（Ｆｅ）、炭素（Ｃ）、バナジウム（Ｖ）及びタングステン（Ｗ）からなる群から選ばれる１種以上の元素を含有していてもよい。
前記粗化処理工程によって形成される粗化処理面の表面粗さＲｚ及び厚さの好ましい範囲は、［電解銅箔の表面検査方法］において説明した電解銅箔の好ましい範囲と同じである。
また、粗化処理工程後には、要求品質に応じて、防錆処理等の表面処理を適宜実施してもよい。
Next, the untreated electrolytic copper foil is roughened.
The roughening treatment is performed by, for example, a plating method in which an electrolytic solution such as copper sulfate is electrolyzed to uniformly precipitate roughened particles containing copper on the matte surface (concave surface) side of the untreated electrolytic copper foil. Can be done. More specifically, an untreated electrolytic copper foil is used as a cathode, an insoluble anode is placed at the counter electrode, and a copper plating solution such as copper sulfate having a liquid temperature of 20 to 40 ° C. is used, and an average anode current density is 5 A / dm. By electrolyzing under the condition of 2 to 40 A / dm 2 , roughened particles can be precipitated on the matte surface of the untreated electrolytic copper foil. Further, the above operation may be performed a plurality of times as needed.
The roughened particles formed by the roughening treatment step usually contain copper, and as elements other than copper, molybdenum (Mo), nickel (Ni), cobalt (Co), iron (Fe), and carbon. It may contain one or more elements selected from the group consisting of (C), vanadium (V) and tungsten (W).
The preferred range of the surface roughness Rz and the thickness of the roughened surface formed by the roughening treatment step is the same as the preferable range of the electrolytic copper foil described in [Method for inspecting the surface of the electrolytic copper foil].
Further, after the roughening treatment step, surface treatment such as rust prevention treatment may be appropriately carried out according to the required quality.
＜検査工程＞
検査工程は、粗化処理工程で得られた粗化処理後の電解銅箔に対して、前記本実施形態の電解銅箔の表面検査方法を実施して良否を判定する工程である。良否の判定は、事前に決定した基準に基づいて実施すればよく、例えば、製造ロットごとに、所定の面積の電解銅箔を切り出し、切り出した面積内において、本実施形態の電解銅箔の表面検査方法によって粗化異常部の個数を計測し、所定の基準を満たしたものを、「良」と判定し、満たさなかったものを「否」と判定することができる。
<Inspection process>
The inspection step is a step of performing the surface inspection method of the electrolytic copper foil of the present embodiment on the electrolytic copper foil after the roughening treatment obtained in the roughening treatment step to determine the quality. The judgment of quality may be carried out based on a predetermined standard. For example, an electrolytic copper foil having a predetermined area is cut out for each production lot, and the surface of the electrolytic copper foil of the present embodiment is within the cut out area. The number of abnormal roughening portions can be measured by an inspection method, and those satisfying a predetermined standard can be determined as "good", and those not satisfying the predetermined criteria can be determined as "no".
以下、実施例を示し、本発明について具体的に説明するが、本発明はこれらに限定されるものではない。 Hereinafter, the present invention will be specifically described with reference to Examples, but the present invention is not limited thereto.
実施例１
（検査対象の準備）
検査対象の電解銅箔として、市販品である、厚さ１８μｍのプリント配線板用電解銅箔（表面粗さＲｚ：７±１．５μｍ）と、厚さ３５μｍのプリント配線板用電解銅箔（表面粗さＲｚ：８．５±１．５μｍ）の２種類を、各々５ロットずつ準備をした。さらに、各ロットの任意の位置から、Ａ４サイズ（２１０ｍｍ×２９７ｍｍ）を２枚ずつ切り出して、これらを試験サンプルとした。
Example 1
(Preparation for inspection)
The electrolytic copper foils to be inspected are commercially available electrolytic copper foils for printed wiring boards with a thickness of 18 μm (surface roughness Rz: 7 ± 1.5 μm) and electrolytic copper foils for printed wiring boards with a thickness of 35 μm (surface roughness Rz: 7 ± 1.5 μm). Two types of surface roughness Rz (8.5 ± 1.5 μm) were prepared for each of 5 lots. Further, two A4 sizes (210 mm × 297 mm) were cut out from arbitrary positions in each lot, and these were used as test samples.
（塗膜形成工程）
上記で準備した試験サンプルの粗化処理面上に、粗化異常部観察用物質として、オイル（呉工業株式会社製、商品名：ＣＲＣ－５５６、鉱物油を主成分として含むオイル）を噴霧して、試験サンプルの粗化処理面全体が均一に濡れるように塗膜）を形成した。
(Coating film forming process)
Oil (manufactured by Kure Engineering Co., Ltd., trade name: CRC-556, oil containing mineral oil as a main component) is sprayed on the roughened surface of the test sample prepared above as a substance for observing abnormal roughening. A coating film was formed so that the entire roughened surface of the test sample was uniformly wetted.
（検査工程）
上記で塗膜を形成した試験サンプルの塗膜形成面を、実体顕微鏡（倍率：１５倍）を用いて観察して、粗化異常部（正常な部分と色調又は形状が異なっている箇所）の数を目視で計測した。評価結果を表１に示す。なお、表１における粗化異常部の個数は、Ａ４サイズの試験サンプル２枚当たりに含まれる粗化異常部の個数である。
(Inspection process)
Observe the coating film-forming surface of the test sample on which the coating film was formed above using a stereomicroscope (magnification: 15 times), and observe the roughened abnormal part (the part where the color tone or shape is different from the normal part). The number was measured visually. The evaluation results are shown in Table 1. The number of abnormal roughening portions in Table 1 is the number of abnormal roughening portions contained in two A4 size test samples.
比較例１
実施例１において、塗膜形成工程を実施しなかったことを以外は、実施例１と同様にして、検査を実施した。
Comparative Example 1
The inspection was carried out in the same manner as in Example 1 except that the coating film forming step was not carried out in Example 1.
表１より、本発明の検査方法である実施例１では、塗膜形成工程を行わずに粗化処理面を観察した比較例１では検出できなかった粗化異常部を検出されており、電解銅箔の粗化処理面に発生する粗化異常部を容易かつ高精度で検出できることが分かる。
また、図１及び２には、実施例１及び比較例１で得られた、粗化処理面を有する電解銅箔の実体顕微鏡画像（（ａ）視野１、（ｂ）視野２）を各々示した。図１から明らかなように、本実施形態の検査方法で得られた実体顕微鏡画像においては、粗化異常部が正常な部分とは大きく異なって見えるため、粗化異常部の検出を容易にできることが分かる。
From Table 1, in Example 1 which is the inspection method of the present invention, an abnormal roughening portion which could not be detected in Comparative Example 1 in which the roughened surface was observed without performing the coating film forming step was detected, and electrolysis was performed. It can be seen that the roughened abnormal portion generated on the roughened surface of the copper foil can be detected easily and with high accuracy.
Further, FIGS. 1 and 2 show stereomicroscopic images ((a) field of
１ 粗化処理面
２ 粗化異常部
1
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